CN109134198A - A kind of method of separation of extractive distillation tetrafluoropropanol and water azeotropic mixture - Google Patents
A kind of method of separation of extractive distillation tetrafluoropropanol and water azeotropic mixture Download PDFInfo
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- CN109134198A CN109134198A CN201811325593.3A CN201811325593A CN109134198A CN 109134198 A CN109134198 A CN 109134198A CN 201811325593 A CN201811325593 A CN 201811325593A CN 109134198 A CN109134198 A CN 109134198A
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- tetrafluoropropanol
- extractive distillation
- extractant
- distillation column
- water
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C29/00—Preparation of compounds having hydroxy or O-metal groups bound to a carbon atom not belonging to a six-membered aromatic ring
- C07C29/74—Separation; Purification; Use of additives, e.g. for stabilisation
- C07C29/76—Separation; Purification; Use of additives, e.g. for stabilisation by physical treatment
- C07C29/80—Separation; Purification; Use of additives, e.g. for stabilisation by physical treatment by distillation
- C07C29/84—Separation; Purification; Use of additives, e.g. for stabilisation by physical treatment by distillation by extractive distillation
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07D—HETEROCYCLIC COMPOUNDS
- C07D207/00—Heterocyclic compounds containing five-membered rings not condensed with other rings, with one nitrogen atom as the only ring hetero atom
- C07D207/02—Heterocyclic compounds containing five-membered rings not condensed with other rings, with one nitrogen atom as the only ring hetero atom with only hydrogen or carbon atoms directly attached to the ring nitrogen atom
- C07D207/18—Heterocyclic compounds containing five-membered rings not condensed with other rings, with one nitrogen atom as the only ring hetero atom with only hydrogen or carbon atoms directly attached to the ring nitrogen atom having one double bond between ring members or between a ring member and a non-ring member
- C07D207/22—Heterocyclic compounds containing five-membered rings not condensed with other rings, with one nitrogen atom as the only ring hetero atom with only hydrogen or carbon atoms directly attached to the ring nitrogen atom having one double bond between ring members or between a ring member and a non-ring member with hetero atoms or with carbon atoms having three bonds to hetero atoms with at the most one bond to halogen, e.g. ester or nitrile radicals, directly attached to ring carbon atoms
- C07D207/24—Oxygen or sulfur atoms
- C07D207/26—2-Pyrrolidones
- C07D207/263—2-Pyrrolidones with only hydrogen atoms or radicals containing only hydrogen and carbon atoms directly attached to other ring carbon atoms
- C07D207/267—2-Pyrrolidones with only hydrogen atoms or radicals containing only hydrogen and carbon atoms directly attached to other ring carbon atoms with only hydrogen atoms or radicals containing only hydrogen and carbon atoms directly attached to the ring nitrogen atom
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- Organic Chemistry (AREA)
- Pyrrole Compounds (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The present invention relates to the methods of a kind of separation of extractive distillation tetrafluoropropanol and water azeotropic mixture, belong to the separation technology field of tetrafluoropropanol and water.The extracting rectifying process uses double-column process, it is made of extractive distillation column and solvent recovery tower, tetrafluoropropanol and aqueous mixtures are introduced from extractive distillation column middle and upper part, it is introduced using N-Methyl pyrrolidone as extractant from the top of tower, after extractive distillation column, water is produced from extracting rectifying tower top, tetrafluoropropanol and extractant introduce in the middle part of solvent recovery tower after the extraction of extractive distillation column tower bottom, tetrafluoropropanol is recycled after being produced by solvent recovery tower tower bottom from solvent recovery tower overhead extraction, extractant N-Methyl pyrrolidone.The method of the invention simple process and low cost, easily operated, product purity is greater than 99.9% after processing, can carry out industrial applications.
Description
Technical field
The invention belongs to chemical separating purification arts, are related to the side of a kind of separation of extractive distillation tetrafluoropropanol and water azeotropic mixture
Method.
Background technique
Tetrafluoropropanol is a kind of important industrial chemicals, it has good dissolubility, non-corrosive, and excellent surface is living
Property and bioactivity.It is widely used to pharmacy, pesticide, surfactant, detergent and solvent, especially in DVD-R or CD-
In the production of R CD, due to its hypotoxicity, used as a kind of important detergent.In general, in cleaning DVD-R or CD-R
CD after, a certain amount of water can be added in tetrafluoropropanol solvent, in order to recycle tetrafluoropropanol, steaming should be passed through
Mixture of the fraction from tetrafluoropropanol and water.However, tetrafluoropropanol and water can form binary azeotrope at 92.5 DEG C, wherein
The molar fraction of 0.267(containing tetrafluoropropanol), this is difficult the tetrafluoropropanol by commonly distilling isolated high-purity.
Patent (CN102976897A) relates to a kind of method for testing salt distillation separating-purifying tetrafluoropropanol.Patent
(CN102718630A) it is reported in and entrainer is added into the thick tetrafluoropropanol containing isobutanol impurity, azeotropic distillation purifies tetrafluoro
Propyl alcohol, but the addition of entrainer can make product contain entrainer, influence application and entrainer poison of the tetrafluoropropanol in terms of medicine
Property is big, inflammable, threatens to the safety of operator.
There is no report using the method for separation of extractive distillation purification tetrafluoropropanol in document at present, the present invention proposes that one kind is adopted
It is easy to operate with traditional extractant, the extraction rectifying method of industrial applications can be carried out.
Summary of the invention
[technical problems to be solved]
The object of the present invention is to provide one kind not to introduce entrainer, product purity height, separation tetrafluoropropanol and water easy to operate
Method.
[technical solution]
The purpose of the present invention is what is be achieved through the following technical solutions.
A kind of method of separation of extractive distillation tetrafluoropropanol and water azeotropic mixture, steps of the method are tetrafluoropropanol and water are mixed
It closes object to enter extractive distillation column (T1) from middle and upper part, extractant enters extractive distillation column (T1) from top, by extractive distillation column
After rectifying, from extracting rectifying tower top (D) recovered water, produce tetrafluoropropanol and extractant from extractive distillation column tower bottom (W), then into
Enter in the middle part of solvent recovery tower (T2), carry out the separation of tetrafluoropropanol and extractant, tetrafluoropropanol is from solvent recovery column overhead (D1)
Extraction, extractant are recycled after being produced by solvent recovery tower tower bottom (S)；This method is using N-Methyl pyrrolidone as extraction
Agent carries out extracting rectifying operation, and the operating condition of extractive distillation column is normal pressure, the mixture material of tetrafluoropropanol and water with room temperature,
1.3 times of atmospheric pressure chargings, extractant are fed with room temperature, 1.3 times of atmospheric pressure；It the use of the water purity that this method obtains is 99.31%-
99.82%, product tetrafluoropropanol purity is 99.97%-99.99%, and extractant purity is 99.96%-99.99%.
According to another preferred embodiment of the present invention, it is characterised in that: extractant mole dosage is mixture material use
2.6-4.2 times of amount.
According to another preferred embodiment of the present invention, it is characterised in that: the temperature of extractive distillation column tower reactor is preferably
172.4-212.4℃。
According to another preferred embodiment of the present invention, it is characterised in that: the number of theoretical plate of extractive distillation column (T1) is 77-
88, reflux ratio 2.2-5.2, the number of plates of solvent recovery tower (T2) are 20-45, reflux ratio 1.5-8.4.
According to another preferred embodiment of the present invention, it is characterised in that: the mixture material of tetrafluoropropanol and water, tetrafluoro
The molar fraction of propyl alcohol is 0.1-0.7, and the molar fraction of water is 0.3-0.9.
[beneficial effect]
The present invention compared with prior art, mainly have it is following the utility model has the advantages that
(1) this method has easy to operate, the high advantage of product purity.
(2) isolated extractant is with high purity and can be recycled, and reduces cost, reduces the influence to environment, just
In industrialized production.
Detailed description of the invention
Attached drawing 1 is tetrafluoropropanol of the invention and laden water separation process flow chart.
T1- extractive distillation column；T2- solvent recovery tower；S- extractive distillation column extractant feed；FEED- extractive distillation column is former
Material charging；The charging of W- solvent recovery tower；D- extractive distillation column overhead product；D1- solvent recovery tower overhead product.
Specific embodiment
The present invention further illustrates the effect of separation of extractive distillation tetrafluoropropanol and aqueous systems in conjunction with the accompanying drawings and embodiments, but
The present invention is not limited to the following embodiments, and in the range of not departing from the front and back objective, alternate embodiment is included in this hair
In bright technical scope.
The method of separation of extractive distillation tetrafluoropropanol and water, process flow chart are as shown in Figure 1.Raw material tetrafluoropropanol and water
Mixture is continuously entered in the middle and upper part of extractive distillation column (T1), while extractant N-Methyl pyrrolidone is in extractive distillation column
(T1) top continuously enters, in the interior light component water of extractive distillation column (T1) from overhead extraction, heavy constituent tetrafluoropropanol and extraction
Agent N-Methyl pyrrolidone enters solvent recovery tower (T2), and heavy constituent tetrafluoropropanol is adopted from tower top after solvent recovery tower (T2)
Out, the extractant N-Methyl pyrrolidone of tower bottom extraction recycles, and has been finally reached azeotropic mixture object system's tetrafluoropropanol and water
Separation.
Embodiment 1
Extracting rectifying process as shown in Figure 1.Extractive distillation column T1 has 77 pieces of theoretical plates, extractant N-Methyl pyrrolidone S
It is added from the 5th block of plate, flow 420.0kmol/h, (molar fraction is tetrafluoropropanol 0.100 to the mixture of tetrafluoropropanol and water
With water 0.900) FEED is added from the 37th block of plate, flow 100.0kmol/h.Extractive distillation column T1 is operated under normal pressure, reflux
Than being 2.2, overhead extraction amount is 90.0kmol/h, obtains water in tower top, and tower bottom obtains the mixture W of tetrafluoropropanol and water from the
20 blocks of plates enter solvent recovery tower T2, and solvent recovery tower T2 has 45 pieces of theoretical plates, reflux ratio 8.4, and overhead extraction amount is
10.0kmol/h, tower top obtain tetrafluoropropanol, and tower bottom obtains extractant N-Methyl pyrrolidone.Extracting rectifying column overhead temperatures are
99.97 DEG C, bottom temperature is 212.4 DEG C.After separation: water purity reaches 99.82%, and product tetrafluoropropanol purity reaches 99.97%,
Extractant N-Methyl pyrrolidone purity reaches 99.99%.
Embodiment 2
Extracting rectifying process as shown in Figure 1.Extractive distillation column T1 has 78 pieces of theoretical plates, extractant N-Methyl pyrrolidone S
It is added from the 5th block of plate, flow 380.0kmol/h, (molar fraction is tetrafluoropropanol 0.267 to the mixture of tetrafluoropropanol and water
With water 0.733) FEED is added from the 35th block of plate, flow 100.0kmol/h.Extractive distillation column T1 is operated under normal pressure, reflux
Than being 2.8, overhead extraction amount is 73.3kmol/h, obtains water in tower top, and tower bottom obtains the mixture W of tetrafluoropropanol and water from the
10 blocks of plates enter solvent recovery tower T2, and solvent recovery tower T2 has 25 pieces of theoretical plates, reflux ratio 2.7, and overhead extraction amount is
26.7kmol/h, tower top obtain tetrafluoropropanol, and tower bottom obtains extractant N-Methyl pyrrolidone.Extracting rectifying column overhead temperatures are
99.91 DEG C, bottom temperature is 199.27 DEG C.After separation: water purity reaches 99.61%, and product tetrafluoropropanol purity reaches
99.98%, extractant N-Methyl pyrrolidone purity reaches 99.99%.
Embodiment 3
Extracting rectifying process as shown in Figure 1.Extractive distillation column T1 has 84 pieces of theoretical plates, extractant N-Methyl pyrrolidone S
It is added from the 4th block of plate, flow 380.0kmol/h, (molar fraction is 0.5 He of tetrafluoropropanol to the mixture of tetrafluoropropanol and water
Water 0.5) FEED is added from the 30th block of plate, flow 100.0kmol/h.Extractive distillation column T1 is operated under normal pressure, and reflux ratio is
3.5, overhead extraction amount is 50.0kmol/h, obtains water in tower top, tower bottom obtains the mixture W of tetrafluoropropanol and water from the 10th piece
Plate enters solvent recovery tower T2, and solvent recovery tower T2 has 20 pieces of theoretical plates, reflux ratio 1.5, and overhead extraction amount is
50.0kmol/h, tower top obtain tetrafluoropropanol, and tower bottom obtains extractant N-Methyl pyrrolidone.Extracting rectifying column overhead temperatures are
99.86 DEG C, bottom temperature is 187.82 DEG C.After separation: water purity reaches 99.32%, and product tetrafluoropropanol purity reaches
99.99%, extractant N-Methyl pyrrolidone purity reaches 99.99%.
Embodiment 4
Extracting rectifying process as shown in Figure 1.Extractive distillation column T1 has 88 pieces of theoretical plates, extractant N-Methyl pyrrolidone S
It is added from the 4th block of plate, flow 260.0kmol/h, (molar fraction is tetrafluoropropanol 0.700 to the mixture of tetrafluoropropanol and water
With water 0.300) FEED is added from the 35th block of plate, flow 100.0kmol/h.Extractive distillation column T1 is operated under normal pressure, reflux
Than being 5.2, overhead extraction amount is 29.9kmol/h, obtains water in tower top, and tower bottom obtains the mixture W of tetrafluoropropanol and water from the
15 blocks of plates enter solvent recovery tower T2, and solvent recovery tower T2 has 30 pieces of theoretical plates, reflux ratio 2.0, and overhead extraction amount is
70.0kmol/h, tower top obtain tetrafluoropropanol, and tower bottom obtains extractant N-Methyl pyrrolidone.Extracting rectifying column overhead temperatures are
99.85 DEG C, bottom temperature is 172.40 DEG C.After separation: water purity reaches 99.31%, and product tetrafluoropropanol purity reaches
99.97%, extractant N-Methyl pyrrolidone purity reaches 99.96%.
Claims (5)
1. a kind of method of separation of extractive distillation tetrafluoropropanol and water azeotropic mixture, it is characterised in that: the step of this method is tetrafluoro
Propyl alcohol and aqueous mixtures enter extractive distillation column (T1) from middle and upper part, and extractant enters extractive distillation column (T1) from top, pass through
After extractive distillation column rectifying, from extracting rectifying tower top (D) recovered water, tetrafluoropropanol and extraction are produced from extractive distillation column tower bottom (W)
Agent is taken, subsequently into the middle part of solvent recovery tower (T2), carrying out the separation of tetrafluoropropanol and extractant, tetrafluoropropanol is from solvent recovery
Column overhead (D1) extraction, extractant are recycled after being produced by solvent recovery tower tower bottom (S)；This method uses N- crassitude
Ketone carries out extracting rectifying operation as extractant, and the operating condition of extractive distillation column is normal pressure, the mixture of tetrafluoropropanol and water
Raw material is fed with room temperature, 1.3 times of atmospheric pressure chargings, extractant with room temperature, 1.3 times of atmospheric pressure；The water obtained using this method is pure
Degree is 99.31%-99.82%, and product tetrafluoropropanol purity is 99.97%-99.99%, and extractant purity is 99.96%-99.99%.
2. according to the method for claim 1, it is characterised in that: the extractant mole dosage is mixture material dosage
2.6-4.2 times.
3. according to the method for claim 1, it is characterised in that: the temperature of described extractive distillation column (T1) tower reactor is preferably
172.4-212.4℃。
4. according to the method for claim 1, it is characterised in that: the number of theoretical plate of the extractive distillation column (T1) is 77-
88, reflux ratio 2.2-5.2, the number of plates of solvent recovery tower (T2) are 20-45, reflux ratio 1.5-8.4.
5. according to the method for claim 1, it is characterised in that: the tetrafluoropropanol and aqueous mixtures, tetrafluoropropanol
Molar fraction is 0.1-0.7, and the molar fraction of water is 0.3-0.9.
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| CN201811325593.3A CN109134198A (en) | 2018-11-08 | 2018-11-08 | A kind of method of separation of extractive distillation tetrafluoropropanol and water azeotropic mixture |
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| CN201811325593.3A CN109134198A (en) | 2018-11-08 | 2018-11-08 | A kind of method of separation of extractive distillation tetrafluoropropanol and water azeotropic mixture |
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Cited By (3)
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| CN110028386A (en) * | 2019-05-23 | 2019-07-19 | 山东科技大学 | A method of utilizing hydrophobicity glyoxaline ion liquid extraction and separation tetrafluoropropanol and water |
| CN114262261A (en) * | 2022-01-06 | 2022-04-01 | 万华化学集团股份有限公司 | Separation method of 2-methyl-3-butyne-2-ol crude product |
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| CN114262261A (en) * | 2022-01-06 | 2022-04-01 | 万华化学集团股份有限公司 | Separation method of 2-methyl-3-butyne-2-ol crude product |
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